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PRODUCT ANALYSIS

Major component of rubber


products
Rubber (Polymer)
Oil ( plasticizer)
Carbon black
Inorganic fillers
Other rubber additives

like antioxidant, accelerator,


sulphur etc

Need for Product analysis


Product analysis can be used for routine
quality control as well as development of
new products.
Polymer type
Polymer

content
Filler content
Carbon black
Plasticizer

Chemical Analysis /Instrumental Analysis

Chemical analysis is time consuming.

Modern instruments can provide quick, efficient

and accurate information.

Chemical Analysis

Chemical analysis gives some information about type

of polymer used, quantity of filler and quantity of


plasticiser used in rubber products.

Instrumental Analysis
FTIR

TGA

FOURIER TRASFORM
INFRARED SPECTROMETER

THERMOGRAVIMETRIC
ANALYZER

Chemical Method
Burning Test
Disintegration in Conc.HNO3
Beilstein Test
Elemental Analysis

Nitrogen
Sulphur
Halogen

Burning Test
Materials burn and continues to burn

on removal from the flame


NR, SBR, IR,BR, etc.
Materials burn but extinguishes itself
on removal from the flame
CR

Heat the polymer with con. Nitric acid

Disintegration

NR, IR, SBR, BR

No disintegration

Butyl, silicone,
EPDM

Test for Chlorine( copper wire Test):


This test is useful to identify halogen

(mainly chlorine) containing polymers


Heat a copper wire till

red hot.
Rub hot copper wire on
sample and heat that
copper wire on the
flame
Observe colour of flame.

Test for Halogen

If colour of the Flame turns green, indicate

presence of chlorine containing polymers. Eg. CR


If colour of flame remains unchanged indicates

presence of non halogenated polymers like NR,


EPDM, SBR, NBR, PBR etc

Elemental Analysis
Rubbers mostly contain C and H
Few rubbers contain elements like N, S and
Halogen

Lassaignes test

Small

pieces of rubber sample is treated with


metallic sodium at high temperature.

The

solution is treated with different reagents to


determine the elements present in the material

Elemental analysis (Lassaignes test)


Sodium fusion extract

Nitrogen

Chlorine

Nitrile
rubber,
Polyuretha
ne

Neoprene,
Hypalon

Sulphur

Hypalon

Moisture content
Weighed sample is heated to 100c for 2hrs.

Again weight is noted. From this moisture


content can be calculated.
Moisture content %

weight of sample - weight of sample after 2 hrs x 100


weight of sample

% Oil Plasticizer by Acetone extraction


Acetone extraction gives oil and other acetone

extractable content (sulphur,


accelerator,antioxidant etc) in the rubber
product
Weigh

2.0 gm of the sample and wrapped


in filter paper and keep in a extraction cup.
Add acetone in the round bottom flask .
Extract the specimen continuously for 16 hrs
keeping the temp of solvent at 60 C to 70
C.
After completion of 16 hrs, the sample is
dried and weighed.

Ash content

A weighed specimen is placed in a weighed crucible


and heated in a muffle furnace at 550 0C+ 25 0C.
The mass of residue in the crucible represents the
ash content

Identification of polymer by FTIR


Acetone Extracted sample is used for

anaysis

Most of the physical, thermal, and chemical

properties are dependent on type of


polymer used in rubber product.

Chemical test gives some information


about type of polymer used in rubber
products but exact

FTIR

FOURIER TRASFORM INFRARED SPECTROSCOPY

Quick method.
A nalyse all type of samples like

solids, gases,liquids, organic,


inorganic,
monomers and polymers.

Reference method is needed

Infrared Region
Near Infrared Region : 13000-4000
cm-1
Middle Infra red Region : 4000 200
cm-1
Far Infrared region : 200 10 cm-1

MIDDLE IR REGION is very important

for
ORGANIC COMPOUNDS

FTIR GRAPH

IR Spectrum
The absorption peaks

Isoprene Rubber

SBR Rubber

Wave number cm-1

Intensity

Wave number cm-1 Intensity

800

699

vs

887

vs

758

885

909

909

962

1370

990

1640

1490

FTIR

GRAPH

TGA Thermo-gravimetric Analyzer

TGA analysis of rubber products


First the volatile materials are lost under nitrogen
purge(upto 300c )followed by rubber in the temperature
range of 300c 550c.
After 550c nitrogen purging is changed to oxygen so that
carbon black is oxidised as indicated by further weight
loss.
The remaining residue is ash which generally comes from
zinc oxide and other inorganic filler and additives

Thermo gram for Calcium


Oxalate
CaC2O4H2O ->

CaC2O4 -> CaCO3 -> CaO

Thank you

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